CN105088345B - A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker - Google Patents
A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker Download PDFInfo
- Publication number
- CN105088345B CN105088345B CN201510449490.8A CN201510449490A CN105088345B CN 105088345 B CN105088345 B CN 105088345B CN 201510449490 A CN201510449490 A CN 201510449490A CN 105088345 B CN105088345 B CN 105088345B
- Authority
- CN
- China
- Prior art keywords
- desert sand
- whisker
- mullite
- preparation
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention discloses a kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker, uses Desert Sand, aluminium hydroxide, bauxite for primary raw material, additional AlF3And V2O5For additive, through dispensing, dry grinding co-grinding, sieve, bury burning and obtain mullite crystal whisker.The present invention significantly reduces the preparation cost of mullite crystal whisker and has promoted the comprehensive utilization of resources of Desert Sand, therefore the present invention has larger economy and social value.
Description
Technical field
The invention belongs to inorganic non-metallic material（Ceramics）Field, and in particular to one kind is not come using the synthesis of Desert Sand low temperature
The preparation method of stone crystal whisker.
Background technology
Science and technology is developed rapidly, and the demand to material property improves increasingly, and traditional simple phase material has been difficult to meet
The actual demand of society, and composite can be applied in wider many fields because having many more excellent performances, by
Many national attention have been arrived, have encouraged material science worker that various composites are carried out with thoroughgoing and painstaking exploration.Whisker
It is that recognized by people, it is prepared and application study turns into field of compound material as one of in composite three big reinforcements
The focus of research.The definition of whisker is a kind of mono-crystlling fibre material, with manual control condition.The diameter of whisker is very small, former
Son distribution very well ordered, internally crystal structure is more complete, and the defect often presented in the big crystal of receiving is very difficult, so not having
Internal structural defects, or only few defects, thus whisker intensity close to the theoretical strength value of crystal, show it
Excellent physics, chemical property and splendid mechanical performance, can be used as ceramics, the reinforcing material of metal.
Mullite (3Al2O3.2SiO2) it is Al2O3-SiO2Compound only stable in system, with high temperature resistant, antioxygen
Change, wear-resistant, thermal coefficient of expansion is small, and thermal shock resistance is good and high-temerature creep is small, less dielectric properties and preferable translucency
Deng excellent properties, it is widely used in the fields such as refractory material, high temperature and engineering material.Mullite crystal whisker not only possesses mullite
The excellent properties of itself, and be that the big complete monocrystal of draw ratio has excellent mechanical property.In addition mullite exists
Oxidizing atmosphere, reducing atmosphere and can be stable when 1700 DEG C of high temperature, anti-strong acid and strong base corrodes, so mullite crystal whisker is
A kind of excellent composite material reinforcement body, can greatly improve Metal Substrate and the combination property of ceramic matric composite.Therefore,
Development and exploitation of the mullite crystal whisker material to promotion new ceramics base and refractory material, increase the material such as advanced ceramics and high-performance
The application development of material is significant.
At present, the method for mullite synthesizing whisker mainly has：Wet chemistry method, include sol-gel process, coprecipitation,
Particle coating technology, spray pyrolysis, Hydrolyze method, hydrothermal crystallization method etc.；Electric smelting method；Sintering process and synthesis by solid state reaction etc..
In numerous synthetic methods, wet chemistry method is mainly used in synthesizing high-purity mullite, and three kinds of methods are then to be used to synthesize below
Industrial mullite.In these methods, although wet chemical method synthesis temperature in mullite synthesizing whisker is relatively low, used
Raw material all based on the higher industrial chemicals of purity；And sintering process and synthesis by solid state reaction are in mullite synthesizing whisker
Synthesis temperature is higher.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation side of utilization Desert Sand low temperature mullite synthesizing whisker
Method.
In order to solve the above technical problems, the technical scheme is that：One kind is brilliant using Desert Sand low temperature mullite synthesizing
The preparation method of palpus, it is characterised in that：Desert Sand, aluminium hydroxide, bauxite are used for primary raw material, additional AlF3And V2O5For
Additive, through dispensing, dry grinding co-grinding, sieve, bury burning obtain mullite crystal whisker.
The Desert Sand, aluminium hydroxide+bauxite, AlF3、V2O5Chemical composition percentage by weight be：Desert Sand：25~
60%th, aluminium hydroxide+bauxite：40~75%, AlF3：2~5%, V2O5：1~6%.
The Ball-milling Time of the dry grinding co-grinding process is 1~3h.
It is described bury burn process calcining system be from room temperature to 1170~1350 DEG C, and 1000 DEG C be incubated 1h,
Maximum temperature soaking time is 1~2h.
It is described to be heated up from room temperature~1170~1350 DEG C with 3~5 DEG C/min speed.
The screen number of the sieving process is 200 mesh.
Using mullite as principal crystalline phase in the microstructure of the mullite crystal whisker, quartz or corundum are time crystalline phase.
The draw ratio of the mullite crystal whisker is 15~140.
The chemical composition of the Desert Sand is as follows：
This patent is from aluminium hydroxide and natural mineral raw bauxite using In Natural Silicate waste salt Desert Sand as silicon source
Silicon source, the mullite synthesizing whisker under 1170-1350 DEG C of low temperature.Desert Sand wide material sources, it is with low cost, utilize Desert Sand and day
Right raw mineral materials prepares mullite crystal whisker, has saved production cost, has taken full advantage of land resource, has had larger to environmental protection
Help, provide a set of new idea and method for the recycling of Desert Sand, have to environmental protection and sustainable development
Larger meaning.
Brief description of the drawings
Fig. 1 is the XRD diffracting spectrums of the sample of embodiment 3；
Fig. 2 is the SEM spectrum of the sample of embodiment 3；
Fig. 3 is the XRD diffracting spectrums of the sample of embodiment 9；
Fig. 4 is the SEM spectrum of the sample of embodiment 9.
Embodiment
Embodiment 1：
By Desert Sand 55%, aluminium hydroxide 45%, additional AlF3 5%、V2O5 After 2% weighing, raw material through 3h dry grind co-grinding,
Cross after 200 mesh sieves, heated up in room temperature~1300 DEG C with 5 DEG C/min speed, be incubated 1h at 1000 DEG C, maximum sintering temperature is 1300
DEG C, maximum temperature soaking time is 2h, and the mullite crystal whisker that draw ratio is 73 is obtained after natural cooling.
Embodiment 2：
By Desert Sand 45%, aluminium hydroxide 55%, additional AlF3 3%、V2O5 After 4% weighing, raw material through 2h dry grind co-grinding,
Cross after 200 mesh sieves, heated up in room temperature~1250 DEG C with 3 DEG C/min speed, be incubated 1h at 1000 DEG C, maximum sintering temperature is 1250
DEG C, maximum temperature soaking time is 1.5h, and the mullite crystal whisker that draw ratio is 115 is obtained after natural cooling.
Embodiment 3：
By Desert Sand 35%, aluminium hydroxide 65%, additional AlF3 4%、V2O5 After 5% weighing, raw material is through 1.5h dry grinding mixed powders
After broken, 200 mesh sieves excessively, heated up in room temperature~1170 DEG C with 3 DEG C/min speed, 1h are incubated at 1000 DEG C, maximum sintering temperature is
1170 DEG C, maximum temperature soaking time is 1h, and the mullite crystal whisker that draw ratio is 140 is obtained after natural cooling.
Embodiment 4：
By Desert Sand 50%, aluminium hydroxide 10%, bauxite 40%, additional AlF3 4%、V2O5 After 4% weighing, raw material is through 2.5h
Dry grind after co-grinding, 200 mesh sieves excessively, heated up in room temperature~1280 DEG C with 4 DEG C/min speed, 1h, highest are incubated at 1000 DEG C
Firing temperature is 1280 DEG C, and maximum temperature soaking time is 2h, and the mullite crystal whisker that draw ratio is 55 is obtained after natural cooling.
Embodiment 5：
By Desert Sand 40%, aluminium hydroxide 50%, bauxite 10%, additional AlF3 2%、V2O5 After 6% weighing, raw material is dry through 2h
Grind co-grinding, cross after 200 mesh sieves, heated up in room temperature~1200 DEG C with 3 DEG C/min speed, 1h, most high fever are incubated at 1000 DEG C
It is 1200 DEG C into temperature, maximum temperature soaking time is 1.5h, the mullite crystal whisker that draw ratio is 82 is obtained after natural cooling.
Embodiment 6：
By Desert Sand 25%, aluminium hydroxide 65%, bauxite 10%, additional AlF3 5%、V2O5 After 2% weighing, raw material is dry through 1h
Grind co-grinding, cross after 200 mesh sieves, heated up in room temperature~1350 DEG C with 5 DEG C/min speed, 1h, most high fever are incubated at 1000 DEG C
It is 1350 DEG C into temperature, maximum temperature soaking time is 1.5h, the mullite crystal whisker that draw ratio is 65 is obtained after natural cooling.
Embodiment 7：
By Desert Sand 60%, bauxite 40%, additional AlF3 2%、V2O5 After 6% weighing, raw material is through 1h dry grinding co-grinding, mistake
After 200 mesh sieves, heated up in room temperature~1250 DEG C with 3 DEG C/min speed, be incubated 1h at 1000 DEG C, maximum sintering temperature is 1250
DEG C, maximum temperature soaking time is 1h, and the mullite crystal whisker that draw ratio is 15 is obtained after natural cooling.
Embodiment 8：
By Desert Sand 45%, bauxite 55%, additional AlF3 4%、V2O5 After 3% weighing, raw material is through 2h dry grinding co-grinding, mistake
After 200 mesh sieves, heated up in room temperature~1300 DEG C with 5 DEG C/min speed, be incubated 1h at 1000 DEG C, maximum sintering temperature is 1300
DEG C, maximum temperature soaking time is 2h, and the mullite crystal whisker that draw ratio is 28 is obtained after natural cooling.
Embodiment 9：
By Desert Sand 35%, bauxite 65%, additional AlF3 5%、V2O5 After 1% weighing, raw material is through 3h dry grinding co-grinding, mistake
After 200 mesh sieves, heated up in room temperature~1350 DEG C with 4 DEG C/min speed, be incubated 1h at 1000 DEG C, maximum sintering temperature is 1350
DEG C, maximum temperature soaking time is 2h, and the mullite crystal whisker that draw ratio is 35 is obtained after natural cooling.
Claims (1)
1. a kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker, it is characterised in that：By Desert Sand 35%, hydrogen-oxygen
Change aluminium 65%, additional AlF3 4%、V2O5 After 5% weighing, raw material through 1.5h dry grind co-grinding, cross 200 mesh sieves after, room temperature~
1170 DEG C are heated up with 3 DEG C/min speed, and 1h is incubated at 1000 DEG C, and maximum sintering temperature is 1170 DEG C, maximum temperature soaking time
For 1h, the mullite crystal whisker that draw ratio is 140 is obtained after natural cooling；
The chemical composition percentage of the Desert Sand is constituted：SiO2 75.95%th, Al2O3 12.68%th, Fe2O3 2.08%、
TiO2 0.29%th, CaO 2.09%, MgO 0.72%, Na2O 1.54%, K2O 2.02%, burning lose 2.63%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510449490.8A CN105088345B (en) | 2015-07-28 | 2015-07-28 | A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510449490.8A CN105088345B (en) | 2015-07-28 | 2015-07-28 | A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105088345A CN105088345A (en) | 2015-11-25 |
| CN105088345B true CN105088345B (en) | 2017-09-19 |
Family
ID=54569638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510449490.8A Expired - Fee Related CN105088345B (en) | 2015-07-28 | 2015-07-28 | A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105088345B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104947177B (en) * | 2015-05-29 | 2017-10-20 | 景德镇陶瓷大学 | One kind is without V2O5The method for preparing mullite crystal whisker with gangue and aluminium hydroxide growth in situ under the conditions of dry-pressing |
| CN106396637B (en) * | 2016-09-06 | 2019-12-31 | 景德镇陶瓷大学 | Preparation method of light low-expansion porcelain building ceramic tile and product prepared by preparation method |
| CN106915749B (en) * | 2017-04-07 | 2019-03-01 | 武汉科技大学 | A kind of rod-like mullite-tabular alumina composite granule and preparation method thereof |
| CN108315810B (en) * | 2018-02-24 | 2020-09-22 | 陕西大秦钾业有限公司 | Method for synthesizing mullite whisker by taking kaliophilite as raw material |
| CN111620679B (en) * | 2020-06-16 | 2022-03-08 | 郑州大学 | Method for preparing high-purity mullite material by taking fused silica as silicon source |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4910172A (en) * | 1989-02-08 | 1990-03-20 | The United States Of America As Represented By The Secretary Of The Navy | Preparation of mullite whiskers from AlF3, SiO2, and Al2 O3 powders |
| CN1785893A (en) * | 2005-10-18 | 2006-06-14 | 山东大学 | Preparation method of mullite whiskers |
| CN1884192A (en) * | 2006-05-25 | 2006-12-27 | 武汉科技大学 | Process for preparing mullite crystal whisker by molten salt method |
| CN101122049A (en) * | 2007-07-25 | 2008-02-13 | 濮阳濮耐高温材料（集团）股份有限公司 | Method for preparing mullite crystal whisker from coal refuse and aluminum oxide |
| CN101775659A (en) * | 2010-01-14 | 2010-07-14 | 陕西理工学院 | Process for preparing mullite whisker or flaky alumina by using coal ash |
| CN101935877A (en) * | 2010-09-03 | 2011-01-05 | 昆明理工大学 | Method for synthesizing mullite whiskers by normal pressure sintering |
| CN102304750A (en) * | 2011-09-20 | 2012-01-04 | 江西旭阳雷迪高科技股份有限公司 | Method for synthesizing mullite whiskers |
| CN102312278A (en) * | 2011-09-20 | 2012-01-11 | 陕西科技大学 | Method for preparing mullite whisker by use of gangue |
-
2015
- 2015-07-28 CN CN201510449490.8A patent/CN105088345B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4910172A (en) * | 1989-02-08 | 1990-03-20 | The United States Of America As Represented By The Secretary Of The Navy | Preparation of mullite whiskers from AlF3, SiO2, and Al2 O3 powders |
| CN1785893A (en) * | 2005-10-18 | 2006-06-14 | 山东大学 | Preparation method of mullite whiskers |
| CN1884192A (en) * | 2006-05-25 | 2006-12-27 | 武汉科技大学 | Process for preparing mullite crystal whisker by molten salt method |
| CN101122049A (en) * | 2007-07-25 | 2008-02-13 | 濮阳濮耐高温材料（集团）股份有限公司 | Method for preparing mullite crystal whisker from coal refuse and aluminum oxide |
| CN101775659A (en) * | 2010-01-14 | 2010-07-14 | 陕西理工学院 | Process for preparing mullite whisker or flaky alumina by using coal ash |
| CN101935877A (en) * | 2010-09-03 | 2011-01-05 | 昆明理工大学 | Method for synthesizing mullite whiskers by normal pressure sintering |
| CN102304750A (en) * | 2011-09-20 | 2012-01-04 | 江西旭阳雷迪高科技股份有限公司 | Method for synthesizing mullite whiskers |
| CN102312278A (en) * | 2011-09-20 | 2012-01-11 | 陕西科技大学 | Method for preparing mullite whisker by use of gangue |
Non-Patent Citations (1)
| Title |
|---|
| 原位合成莫来石晶须及其微观结构的研究;徐晓虹等;《陶瓷学报》;20070630;第28卷(第2期);第89-92页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105088345A (en) | 2015-11-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105088345B (en) | A kind of preparation method of utilization Desert Sand low temperature mullite synthesizing whisker | |
| Wang et al. | Utilization of coal fly ash for the production of glass-ceramics with unique performances: A brief review | |
| CN104328478B (en) | A kind of preparation method of SiC whisker | |
| Wu et al. | Preparation and characterization of ceramic proppants with low density and high strength using fly ash | |
| Chen et al. | Mullite whisker network reinforced ceramic with high strength and lightweight | |
| CN101565323B (en) | Method for preparing microcrystalline glass composite material containing alumina | |
| CN102312278B (en) | Method for preparing mullite whisker by use of gangue | |
| CN111620679A (en) | Method for preparing high-purity mullite material by taking fused silica as silicon source | |
| CN100491250C (en) | Method for preparing mullite from gangue | |
| CN105801064A (en) | Production technology of light-weight and heat-insulation brick | |
| CN102304750A (en) | Method for synthesizing mullite whiskers | |
| CN108675657A (en) | A method of preparing silicate-aluminium sulfate compound system clinker using waste residue | |
| CN102674381A (en) | Method for preparing nano mullite powder from coal-based kaolin | |
| CN103626510B (en) | Method for preparing magnesium borate whisker porous ceramic by employing in-situ growth | |
| CN101531523A (en) | Method for synthesizing mullite through utilization of waste | |
| CN102718521B (en) | Method of using coal gangue to prepare fracturing propping agent | |
| CN101585711A (en) | Utilize useless mud of ceramics factory and commercial alumina to prepare the method for high alumina mullite aggregate | |
| CN103467078B (en) | Preparation method of cordierite material | |
| CN102433583A (en) | Preparation method of mullite whiskers | |
| CN1565973A (en) | Process for preparing high purity superfine Al2O3 powder | |
| CN100491251C (en) | Method for preparing mullite from kaoline | |
| CN102731129B (en) | Method for preparing composite fracturing propping agent by using gold tailings and forsterite fibers | |
| CN101974782B (en) | Method of preparing alpha-Al2O3 crystal whisker by carbothermal reduction | |
| CN103449839A (en) | Composite for manufacturing building blocks and manufacturing method of building blocks | |
| CN102173430B (en) | Technique for preparing wollastonite ultrafine powder from calcium silicate hydrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 333001 Tao Yang Road, Jingdezhen New District, Jiangxi, No. 27 Applicant after: JINGDEZHEN CERAMIC INSTITUTE Address before: 333001 Tao Yang Road, Jingdezhen New District, Jiangxi, No. 27 Applicant before: Jingdezhen College of Ceramic Industry |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170919 Termination date: 20200728 |